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. 2025 Sep;41(9):1058-1066.
doi: 10.1016/j.dental.2025.06.014. Epub 2025 Jun 20.

Physicochemical properties and apatite precipitation behavior of experimental calcium silicate-based cements doped with phosphate compounds

Kenta Tsuchiya  1 , Salvatore Sauro  2 , Hidehiko Sano  3 , Jukka P Matinlinna  4 , Monica Yamauti  5 , Shuhei Hoshika  3 , Yu Toida  3 , Rafiqul Islam  3 , Atsushi Tomokiyo  3
Affiliations

Physicochemical properties and apatite precipitation behavior of experimental calcium silicate-based cements doped with phosphate compounds

Kenta Tsuchiya et al. Dent Mater. 2025 Sep.

Abstract

Objectives: This study aims to evaluate the solubility, pH, Ca2 + release, setting time, and hydroxyapatite (HAp) formation of the tested materials.

Methods: Four study groups were tested: NEX-MTA (NMTA; GC, Japan), NMTA with phosphorylated pullulan (MTA-PPL), NMTA with poly-PS (MTA-polyPS), and Biodentine (BD; Septodont, France). Solubility was measured after 7 and 28 days at 37 °C in deionized water. Ca2+ release and pH evaluation were performed after immersion in deionized water at 3 h, 24 h, 7 days, and 28 days using pH and Ca2+ meters. Setting times were determined with a Vicat apparatus, and apatite precipitation was evaluated through scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/ EDS) and Fourier transform infrared spectroscopy (FTIR) analysis 28 days in phosphate-buffered saline.

Results: NMTA showed the lowest solubility; however, there was no statistically significant difference between NMTA and MTA-polyPS (P > 0.05). NMTA exhibited the most alkaline pH at all measured time points. Although MTA-polyPS consistently showed lower pH values than NMTA throughout the observation periods, no statistically significant differences were observed among MTA-polyPS, BD, and MTA-PPL at 28 days (P > 0.05). BD released the most Ca2+, with MTA-polyPS releasing the least. BD exhibited the shortest initial and final setting time (9.2 and 42 min, respectively), followed by MTA-polyPS, MTA-PPL, and NMTA. SEM/ EDS and FTIR indicated that MTA-polyPS had the highest apatite precipitation, with Ca/P ratios of 1.70 (NMTA) and 1.79 (MTA-polyPS). MTA-PPL and BD showed no significant apatite precipitation, with Ca/P ratios of 3.93 and 34.9, respectively.

Significance: The incorporation of polyPS into calcium silicate-based cement may enhance apatite precipitation and accelerate the setting without altering the pH and solubility property.

Keywords: Bioactivity; Calcium silicate cement; Endodontics; Hydroxyapatite; Mineral trioxide aggregate.

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Conflict of interest statement

Declaration of Competing Interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Kenta Tsuchiya reports article publishing charges was provided by JST SPRING, Grant Number JPMJSP2119. If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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